CN103387252B - Anti-caking high-purity barium hydroxide and preparation method thereof - Google Patents
Anti-caking high-purity barium hydroxide and preparation method thereof Download PDFInfo
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- CN103387252B CN103387252B CN201310328474.4A CN201310328474A CN103387252B CN 103387252 B CN103387252 B CN 103387252B CN 201310328474 A CN201310328474 A CN 201310328474A CN 103387252 B CN103387252 B CN 103387252B
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- barium hydroxide
- air
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- hydrated barta
- agglomeration resistance
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Abstract
The invention provides an anti-caking high-purity barium hydroxide and a preparation method thereof. The method comprises the following steps: (1) preparing a Ba(OH)2 solution; (2) purifying the air; and (3) performing coating treatment: spraying the barium hydroxide solution prepared in the step (1) to treat barium octahydrate with particle diameter being smaller than 4000 microns, and then, cooling the barium octahydrate by using the air purified in the step (2) to the room temperature to obtain an anti-caking barium octahydrate product. The non-caking time of the anti-caking high-purity barium octahydrate product at 45 DEG C is larger than or equal to 43 days, and the barium hydroxide content is 99.50-100.43wt%.
Description
Technical field
The present invention relates to a kind of hydrated barta and preparation method thereof, concrete, relate to a kind of agglomeration resistance High Purity Hydrogen barium oxide and preparation method thereof.
Background technology
High Purity Hydrogen barium oxide is mainly used in the manufacture of the electronic devices and components including chip multilayer ceramic capacitor (MLCC).High-purity barium hydroxide (Ba (OH)
28H
2o) generally adopt the method for crystallisation by cooling to produce.Owing to easily causing hydrated barta product surface dehydration efflorescence in drying course, thereby have influence on downstream client's formula precision.But the barium hydroxide that does not carry out drying and processing very easily lumps, thereby cause application difficult.In the prior art, can adopt the mode of adding anti-hard caking agent to avoid barium hydroxide caking, but the consequence of processing like this can be introduced impurity again in hydrated barta product.As can be seen here, prepare the high-purity barium hydroxide of agglomeration resistance and become industrial hot spot.
Summary of the invention
Technical problem to be solved by this invention is: overcome existing barium hydroxide and very easily lump or adopt anti-hard caking agent processing can introduce the defect of impurity, a kind of agglomeration resistance High Purity Hydrogen barium oxide and preparation method thereof is provided, gained hydrated barta purity is high, and keeps the loose not caking time long.
The purity (content) of barium hydroxide product, in fact has close relationship with caking performance.Because barium hydroxide product is containing crystal water, after drying, content is greater than 100% sometimes, but also can cause product efflorescence, caking.The major cause that causes caking is free-water, thus when the foreign matter content such as strontium in barium hydroxide product low, not efflorescence could solve agglomeration problems again simultaneously.
The present invention adopts at high-purity barium hydroxide (Ba (OH)
28H
2o) the coated High Purity Hydrogen barium oxide solution of surface spraying, the coating layer of forming section dehydration (being less than 8 crystal water), has prepared the high-purity barium hydroxide product of agglomeration resistance, and the caking time does not reach more than 43 days for 45 DEG C of products obtained therefroms.
45 DEG C of the present invention do not lump and refer at 45 DEG C of barium hydroxides apparent loosely, and 45 DEG C of visual inspection barium hydroxides are loose.
In order to solve the problems of the technologies described above, the first technical scheme provided by the invention is, a kind of preparation method of agglomeration resistance hydrated barta, and the method comprises:
(1) Ba (OH)
2solution preparation
By the barium hydroxide solution of 1.5～4.0mol/L be heated to 70-75 DEG C stand-by;
(2) purifying air
Remove the CO containing in air
2gas, the air being purified;
(3) coated processing
Process with step (1) gained barium hydroxide solution spray the barium hydroxide that particle diameter is less than 4000 μ m, then use the air cooling of step (2) gained purification to room temperature, obtain agglomeration resistance barium hydroxide product.
The solution temperature that barium hydroxide particle surface sprays is up higher, and therefore under air purification effect, moisture content can evaporate, thus the coating layer of forming section dehydration (being less than 8 crystal water).
The preparation method of aforesaid agglomeration resistance hydrated barta, in step (3), the barium hydroxide that particle diameter is less than to 4000 μ m is placed on guipure, bed thickness is controlled at and is less than 10mm, guipure rate of advance is controlled at 800～1000mm/min, in the 150-250mm region of guipure working direction, step for barium hydroxide (1) gained barium hydroxide solution is sprayed.
The preparation method of aforesaid agglomeration resistance hydrated barta, in step (1), the concentration of described barium hydroxide solution is 3.0-3.5mol/L.
The preparation method of aforesaid agglomeration resistance hydrated barta, in step (3), the barium hydroxide that described particle diameter is less than 4000 μ m is made by following step: by barium hydroxide solution crystallisation by cooling, obtain crystal and crystalline mother solution, then by crystal centrifuge dehydration, pulverize, obtain the barium hydroxide that particle diameter is less than 4000 μ m.
The preparation method of aforesaid agglomeration resistance hydrated barta, in step (2), adopts crystalline mother solution according to 9-11L/m
2(preferably 10L/m
2) spray flux air is carried out to secondary spray cleaning, to remove the CO containing in air
2gas
The invention provides the second technical scheme is, a kind of agglomeration resistance hydrated barta, 45 DEG C not the caking time be more than or equal to 43 days (being preferably greater than 60 days), hydrated barta content is 99.50-100.43wt%.
The invention provides the 3rd technical scheme is that a kind of agglomeration resistance hydrated barta, is made by aforesaid method.
Aforesaid agglomeration resistance hydrated barta, its 45 DEG C not the caking time be more than or equal to 43 days (being preferably greater than 60 days), hydrated barta content is 99.50-100.43wt%.
Adopt technical scheme of the present invention, at least there is following beneficial effect:
Adopt in the barytic method of high-purity barium hydroxide surface spraying covered section dehydration High Purity Hydrogen, prepared the high-purity barium hydroxide product of agglomeration resistance, its 45 DEG C not the caking time be more than or equal to 43 days, hydrated barta content is 99.50-100.43wt%.
Brief description of the drawings
The process flow sheet that Fig. 1 the present invention is main.
Embodiment
For fully understanding object, feature and effect of the present invention, by following concrete embodiment, the present invention is elaborated.
As shown in Figure 1, a kind of preparation method of agglomeration resistance hydrated barta, the method comprises:
(1) Ba (OH)
2solution preparation
By preferred 1.5～4.0mol/L(3.0-3.5mol/L) barium hydroxide solution be heated to 70-75 DEG C stand-by.
(2) purifying air
Remove the CO containing in air
2gas, the air being purified.
Concrete, adopt the solution (for example remaining crystalline mother solution after barium hydroxide solution crystallization hydrated barta) that contains divalence barium ion according to 9-11L/m
2(preferably 10L/m
2) spray flux air is carried out to secondary spray cleaning, to remove the CO containing in air
2gas." secondary spray " processed in two scavenging tower of series connection and carried out, and air enters the first scavenging tower from the inlet mouth at the bottom of the first scavenging tower tower, in the first scavenging tower, upwards flows; The solution that simultaneously contains divalence barium ion from the mouth spray spray of the first scavenging tower tower top and, absorb airborne carbonic acid gas.Air after purifying treatment is gone out from the pneumatic outlet of the first scavenging tower tower top for the first time, and the inlet mouth at the bottom of the second scavenging tower tower enters the second scavenging tower, in the second scavenging tower, upwards flows; The solution that simultaneously contains divalence barium ion from the mouth spray spray of the second scavenging tower tower top and, absorb airborne carbonic acid gas, complete for the second time and purify.
(3) coated processing
Process with step (1) gained barium hydroxide solution spray the barium hydroxide that particle diameter is less than 4000 μ m, then use the air cooling of step (2) gained purification to room temperature, obtain agglomeration resistance barium hydroxide product.
Concrete, the barium hydroxide that particle diameter is less than to 4000 μ m is placed on guipure, bed thickness is controlled at and is less than 10mm, guipure rate of advance is controlled at 800～1000mm/min, at the preferred 200mm of the 150-250mm(of guipure working direction) region sprays step for barium hydroxide (1) gained barium hydroxide solution, then use the air cooling of step (2) gained purification to room temperature, obtain agglomeration resistance barium hydroxide product.
The barium hydroxide that described particle diameter is less than 4000 μ m is made by following step: by barium hydroxide solution crystallisation by cooling, obtain crystal and crystalline mother solution, then by crystal centrifuge dehydration, pulverize, obtain the barium hydroxide that particle diameter is less than 4000 μ m.
Above-mentioned barium hydroxide solution can be made by solubility divalence barium salt and alkali substance reaction, also can be dissolved and be obtained by commercially available hydrated barta.Solubility divalence barium salt is bariumchloride, barium sulphide or barium hydrosulfide.Alkaline matter is sodium hydroxide, potassium hydroxide or Manganse Dioxide.
The agglomeration resistance hydrated barta of being prepared by aforesaid method, 45 DEG C not the caking time be more than or equal to 43 days (being preferably greater than 60 days), hydrated barta content is 99.50-100.43wt%.
Set forth the enforcement of method of the present invention below by specific embodiment, one skilled in the art will appreciate that this should not be understood to the restriction to the claims in the present invention scope.
Embodiment
Embodiment 1
(1) barium hydroxide raw materials pretreatment
By analytical pure barium hydroxide solution, at 40 DEG C of crystallisation by cooling, centrifuge dehydration, obtains crystallization and crystalline mother solution, and gained crystallization is Ba (OH)
28H
2o.Then use ceramic crusher by gained crystallization fragmentation, cross 5 mesh sieves (4.0mm), obtain pretreated barium hydroxide raw material.
(2) Ba (OH)
2solution preparation
Adopt analytical pure hydrated barta, it is mixed with to [Ba with pure water
2+] be the barium hydroxide solution of 1.5mol/L, be then heated to 70 DEG C stand-by.
(3) purifying air
By (1) barium hydroxide feed pretreatment step gained crystalline mother solution according to 9L/m
2spray flux air is carried out to secondary spray cleaning, to remove the CO containing in air
2gas." secondary spray " processed in two scavenging tower of series connection and carried out, and air enters the first scavenging tower from the inlet mouth at the bottom of the first scavenging tower tower, in the first scavenging tower, upwards flows; The solution that simultaneously contains divalence barium ion from the mouth spray spray of the first scavenging tower tower top and, absorb airborne carbonic acid gas.Air after purifying treatment is gone out from the pneumatic outlet of the first scavenging tower tower top for the first time, and the inlet mouth at the bottom of the second scavenging tower tower enters the second scavenging tower, in the second scavenging tower, upwards flows; The solution that simultaneously contains divalence barium ion from the mouth spray spray of the second scavenging tower tower top and, absorb airborne carbonic acid gas, complete for the second time and purify.
(4) coated processing
The pretreated barium hydroxide raw material of step (1) gained is placed on stainless steel guipure, bed thickness is controlled at and is less than 10mm, guipure rate of advance is controlled at 1000mm/min, in the 200mm region of guipure working direction, step for barium hydroxide (2) gained barium hydroxide solution is sprayed, then use the air cooling of step (3) gained purification to room temperature, obtain agglomeration resistance barium hydroxide product 1#.
Embodiment 2
(1) barium hydroxide raw materials pretreatment
By analytical pure barium hydroxide solution, at 40 DEG C of crystallisation by cooling, centrifuge dehydration, obtains crystallization and crystalline mother solution, and gained crystallization is Ba (OH)
28H
2o.Then use ceramic crusher by gained crystallization fragmentation, cross 5 mesh sieves (4.0mm), obtain pretreated barium hydroxide raw material.
(2) Ba (OH)
2solution preparation
Adopt analytical pure hydrated barta, it is mixed with to [Ba with pure water
2+] be the barium hydroxide solution of 3.0mol/L, be then heated to 72 DEG C stand-by.
(3) purifying air
By (1) barium hydroxide feed pretreatment step gained crystalline mother solution according to 11L/m
2spray flux air is carried out to secondary spray cleaning, to remove the CO containing in air
2gas." secondary spray " processed in two scavenging tower of series connection and carried out, and air enters the first scavenging tower from the inlet mouth at the bottom of the first scavenging tower tower, in the first scavenging tower, upwards flows; The solution that simultaneously contains divalence barium ion from the mouth spray spray of the first scavenging tower tower top and, absorb airborne carbonic acid gas.Air after purifying treatment is gone out from the pneumatic outlet of the first scavenging tower tower top for the first time, and the inlet mouth at the bottom of the second scavenging tower tower enters the second scavenging tower, in the second scavenging tower, upwards flows; The solution that simultaneously contains divalence barium ion from the mouth spray spray of the second scavenging tower tower top and, absorb airborne carbonic acid gas, complete for the second time and purify.
(4) coated processing
The pretreated barium hydroxide raw material of step (1) gained is placed on stainless steel guipure, bed thickness is controlled at and is less than 10mm, guipure rate of advance is controlled at 900mm/min, in the 200mm region of guipure working direction, step for barium hydroxide (2) gained barium hydroxide solution is sprayed, then use the air cooling of step (3) gained purification to room temperature, obtain agglomeration resistance barium hydroxide product 2#.
Embodiment 3
(1) barium hydroxide raw materials pretreatment
By analytical pure barium hydroxide solution, at 40 DEG C of crystallisation by cooling, centrifuge dehydration, obtains crystallization and crystalline mother solution, and gained crystallization is Ba (OH)
28H
2o.Then use ceramic crusher by gained crystallization fragmentation, cross 5 mesh sieves (4.0mm), obtain pretreated barium hydroxide raw material.
(2) Ba (OH)
2solution preparation
Adopt analytical pure hydrated barta, it is mixed with to [Ba with pure water
2+] be the barium hydroxide solution of 3.5mol/L, be then heated to 72 DEG C stand-by.
(3) purifying air
By (1) barium hydroxide feed pretreatment step gained crystalline mother solution according to 10L/m
2spray flux air is carried out to secondary spray cleaning, to remove the CO containing in air
2gas." secondary spray " processed in two scavenging tower of series connection and carried out, and air enters the first scavenging tower from the inlet mouth at the bottom of the first scavenging tower tower, in the first scavenging tower, upwards flows; The solution that simultaneously contains divalence barium ion from the mouth spray spray of the first scavenging tower tower top and, absorb airborne carbonic acid gas.Air after purifying treatment is gone out from the pneumatic outlet of the first scavenging tower tower top for the first time, and the inlet mouth at the bottom of the second scavenging tower tower enters the second scavenging tower, in the second scavenging tower, upwards flows; The solution that simultaneously contains divalence barium ion from the mouth spray spray of the second scavenging tower tower top and, absorb airborne carbonic acid gas, complete for the second time and purify.
(4) coated processing
The pretreated barium hydroxide raw material of step (1) gained is placed on stainless steel guipure, bed thickness is controlled at and is less than 10mm, guipure rate of advance is controlled at 900mm/min, in the 200mm region of guipure working direction, step for barium hydroxide (2) gained barium hydroxide solution is sprayed, then use the air cooling of step (3) gained purification to room temperature, obtain agglomeration resistance barium hydroxide product 3#.
Embodiment 4
(1) barium hydroxide raw materials pretreatment
By analytical pure barium hydroxide solution, at 40 DEG C of crystallisation by cooling, centrifuge dehydration, obtains crystallization and crystalline mother solution, and gained crystallization is Ba (OH)
28H
2o.Then use ceramic crusher by gained crystallization fragmentation, cross 5 mesh sieves (4.0mm), obtain pretreated barium hydroxide raw material.
(2) Ba (OH)
2solution preparation
Adopt analytical pure hydrated barta, it is mixed with to [Ba with pure water
2+] be the barium hydroxide solution of 4.0mol/L, be then heated to 75 DEG C stand-by.
(3) purifying air
By (1) barium hydroxide feed pretreatment step gained crystalline mother solution according to 11L/m
2spray flux air is carried out to secondary spray cleaning, to remove the CO containing in air
2gas." secondary spray " processed in two scavenging tower of series connection and carried out, and air enters the first scavenging tower from the inlet mouth at the bottom of the first scavenging tower tower, in the first scavenging tower, upwards flows; The solution that simultaneously contains divalence barium ion from the mouth spray spray of the first scavenging tower tower top and, absorb airborne carbonic acid gas.Air after purifying treatment is gone out from the pneumatic outlet of the first scavenging tower tower top for the first time, and the inlet mouth at the bottom of the second scavenging tower tower enters the second scavenging tower, in the second scavenging tower, upwards flows; The solution that simultaneously contains divalence barium ion from the mouth spray spray of the second scavenging tower tower top and, absorb airborne carbonic acid gas, complete for the second time and purify.
(4) coated processing
The pretreated barium hydroxide raw material of step (1) gained is placed on stainless steel guipure, bed thickness is controlled at and is less than 10mm, guipure rate of advance is controlled at 1000mm/min, in the 200mm region of guipure working direction, step for barium hydroxide (2) gained barium hydroxide solution is sprayed, then use the air cooling of step (3) gained purification to room temperature, obtain agglomeration resistance barium hydroxide product 4#.
Through ultimate analysis and 45 DEG C of observations of not luming, the results are shown in Table 1.
Table 1
| Project | Untreated | 1 # | 2 # | 3 # | 4 # |
| Hydrated barta content wt% | 97.63 | 99.50 | 99.63 | 99.87 | 100.43 |
| 45 DEG C do not lump the time (my god) | 17 | 43 | >60 | >60 | >60 |
The present invention adopts at high-purity barium hydroxide (Ba (OH)
28H
2o) the coated dehydration High Purity Hydrogen barium oxide of surface spraying, has prepared the high-purity barium hydroxide product of agglomeration resistance, 45 DEG C of products obtained therefroms not the caking time reach more than 43 days, hydrated barta content is 99.50-100.43wt%.
Claims (9)
1. a preparation method for agglomeration resistance hydrated barta, the method comprises:
(1) Ba (OH)
2solution preparation
By the barium hydroxide solution of 1.5～4.0mol/L be heated to 70-75 DEG C stand-by;
(2) purifying air
Remove the CO containing in air
2gas, the air being purified;
(3) coated processing
Process with step (1) gained barium hydroxide solution spray the barium hydroxide that particle diameter is less than 4000 μ m, then use the air cooling of step (2) gained purification to room temperature, obtain agglomeration resistance barium hydroxide product.
2. the preparation method of agglomeration resistance hydrated barta according to claim 1, it is characterized in that, in step (3), the barium hydroxide that particle diameter is less than to 4000 μ m is placed on guipure, bed thickness is controlled at and is less than 10mm, guipure rate of advance is controlled at 800～1000mm/min, in the 150-250mm region of guipure working direction, step for barium hydroxide (1) gained barium hydroxide solution is sprayed.
3. the preparation method of agglomeration resistance hydrated barta according to claim 1, is characterized in that, in step (1), the concentration of described barium hydroxide solution is 3.0-3.5mol/L.
4. according to the preparation method of the agglomeration resistance hydrated barta described in claim 1-3 any one, it is characterized in that, in step (3), the barium hydroxide that described particle diameter is less than 4000 μ m is made by following step: by barium hydroxide solution crystallisation by cooling, obtain crystal and crystalline mother solution, then by crystal centrifuge dehydration, pulverize, obtain the barium hydroxide that particle diameter is less than 4000 μ m.
5. the preparation method of agglomeration resistance hydrated barta according to claim 4, is characterized in that, in step (2), adopts crystalline mother solution according to 9-11L/m
2spray flux air is carried out to secondary spray cleaning, to remove the CO containing in air
2gas.
6. the preparation method of agglomeration resistance hydrated barta according to claim 5, is characterized in that, in step (2), adopts crystalline mother solution according to preferred 10L/m
2spray flux air is carried out to secondary spray cleaning.
7. an agglomeration resistance barium hydroxide, is characterized in that, is made up of method described in claim 1-5 any one.
8. agglomeration resistance hydrated barta according to claim 7, is characterized in that, its 45 DEG C not the caking time be more than or equal to 43 days, hydrated barta content is 99.50-100.43wt%.
9. agglomeration resistance hydrated barta according to claim 8, is characterized in that, its 45 DEG C the caking time is not greater than 60 days.
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Citations (2)
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|---|---|---|---|---|
| CN102701258A (en) * | 2012-05-21 | 2012-10-03 | 贵州红星发展股份有限公司 | Anti-blocking method of high-purity strontium nitrate used in liquid crystal substrate |
| CN102701257A (en) * | 2012-06-04 | 2012-10-03 | 重庆新申世纪化工有限公司 | Preparation method of anti-blocking strontium chloride |
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|---|---|---|---|---|
| CN102701258A (en) * | 2012-05-21 | 2012-10-03 | 贵州红星发展股份有限公司 | Anti-blocking method of high-purity strontium nitrate used in liquid crystal substrate |
| CN102701257A (en) * | 2012-06-04 | 2012-10-03 | 重庆新申世纪化工有限公司 | Preparation method of anti-blocking strontium chloride |
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| 技术转让与合作;天津化工研究设计院;《化工科技市场》;20011231;第54页左栏最后一行至右栏第1行 * |
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